Surface chemical analysis Secondary-ion mass spectrometry Calibration of the mass scale for a time-of-flight secondary-ion mass spectrometer

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1 BSI Standards Publication Surface chemical analysis Secondary-ion mass spectrometry Calibration of the mass scale for a time-of-flight secondary-ion mass spectrometer

2 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 13084:2011. The UK participation in its preparation was entrusted to T e c h n Committee i c a l CII/60, Surface chemical analysis. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. BSI 2011 ISBN ICS Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May Amendments issued since publication Date T e x t a f f e c t e d

3 INTERNATIONAL STANDARD BS ISO 13084:2011 ISO First edition Surface chemical analysis Secondaryion mass spectrometry Calibration of the mass scale for a time-of-flight secondary-ion mass spectrometer Analyse chimique des surfaces Spectrométrie de masse des ions secondaires Étalonnage de l'échelle de masse pour un spectromètre de masse des ions secondaires à temps de vol Reference number ISO 2011

4 COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel Fax Web Published in Switzerland ii ISO 2011 All rights reserved

5 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 6, Secondary ion mass spectrometry. ISO 2011 All rights reserved iii

6 Introduction Secondary-ion mass spectrometry (SIMS) is a powerful technique for the analysis of organic and molecular surfaces. Over the last decade, instrumentation has improved significantly so that modern instruments now have very high repeatability and constancy (Reference [2] in the Bibliography). An increasing requirement is for the identification of the chemical composition of complex molecules from accurate measurements of the mass of the secondary ions. The relative mass accuracy to do this and to distinguish between molecules that contain different chemical constituents, but are of the same nominal mass (rounded to the nearest integer mass), is thus an important parameter. A relative mass accuracy of better than 10 ppm is required to distinguish between C 2 H 4 (28, u) and Si (27, u) in a parent ion with total mass up to u, and between CH 2 (14, u) and N (14, u) in parent ions with total mass up to 300 u. However, in a recent interlaboratory study (Reference [3] in the Bibliography), the average fractional mass accuracy was found to be 150 ppm. This is significantly worse than is required for unambiguous identification of ions. A detailed study (Reference [4] in the Bibliography) shows that the key factors degrading the accuracy include the large kinetic energy distribution of secondary ions, non-optimized instrument parameters and extrapolation of the mass scale calibration. This International Standard describes a simple method, using locally sourced material, to optimize the instrumental parameters, as well as a procedure to ensure that accurate calibration of the mass scale is achieved within a selectable uncertainty. iv ISO 2011 All rights reserved

7 INTERNATIONAL STANDARD Surface chemical analysis Secondary-ion mass spectrometry Calibration of the mass scale for a time-of-flight secondary-ion mass spectrometer 1 Scope This International Standard specifies a method to optimize the mass calibration accuracy in time-of-flight SIMS instruments used for general analytical purposes. It is only applicable to time-of-flight instruments but is not restricted to any particular instrument design. Guidance is provided for some of the instrumental parameters that can be optimized using this procedure and the types of generic peaks suitable to calibrate the mass scale for optimum mass accuracy. 2 Symbols and abbreviated terms 2.1 Symbols m mass of interest m 1 calibration mass 1 m 2 calibration mass 2 M mass accuracy (u) M P measured peak mass (u) M T true mass (u) U(m) mass uncertainty for a mass m, arising from calibration U 1 uncertainty in the accurate mass measurement of m 1 U 2 uncertainty in the accurate mass measurement of m 2 U 0 average uncertainty in an accurate mass measurement V R reflector or acceptance voltage (V) W relative mass accuracy x number of carbon atoms y number of hydrogen atoms σ( M) standard deviation of the mass accuracy for a number of peaks σ M average of the standard deviations of M for each of the four C x H + y cascades with 4, 6, 7 and 8 carbon atoms 2.2 Abbreviated terms MEMS PC ppm r/min SIMS THF ToF micro-electromechanical system polycarbonate parts per million revolutions per minute secondary-ion mass spectrometry tetrahydrofuran time of flight ISO 2011 All rights reserved 1

8 3 Outline of method Here, the method is outlined so that the detailed procedure, given in Clause 4, may be understood in context. Firstly, to optimize a time-of-flight mass spectrometer using this procedure, obtain a thin film of PC on a conducting substrate (silicon). The optimization procedure is achieved by carrying out the procedures in 4.3 to 4.5 iteratively; it uses 19 specific C x H y peaks in the polycarbonate (PC) positive-ion mass spectrum. In 4.6, a general calibration procedure is given which provides the rules by which calibrations for inorganics and organics may be incorporated. This leads to a new generic set of ions for mass calibration that can improve the mass accuracy from some often used calibrations by a factor of 5. The effects of extrapolation beyond the calibration range are discussed and a recommended procedure is given to ensure that accurate mass is achieved, within a selectable uncertainty, for large molecules. Therefore, the procedure has two parts, optimization and calibration. Subclauses 4.1 to 4.5 are only required as part of the regular maintenance of the instrument as defined by the testing laboratory. Subclause 4.6 is required for all calibrations of the mass scale. This is summarized in the flowchart in Figure 1. START Optimize instrumental parameters? No Yes 4.1/4.2 Obtaining/Preparing the reference sample for optimization 4.3 Obtaining SIMS spectral data 4.4 Calculating mass accuracy 4.5 Optimizing instrumental parameters 4.6 Calibration procedure for spectra Figure 1 Flowchart of sequence of operations of the method 2 ISO 2011 All rights reserved

9 4 Method for improving mass accuracy 4.1 Obtaining the reference sample for optimization A sample of thin (10 to 100 nm) PC on a flat conducting substrate (e.g. silicon wafer) shall either be obtained or prepared, as described at Preparation of polycarbonate sample Instructions for the preparation of a PC reference sample are provided. This method can give sample-to-sample repeatability in ToF SIMS spectra of better than 1,9 % [2]. To prepare such a sample for static SIMS analysis requires a clean working environment. To reduce surface contamination, clean glassware, tweezers and powderless gloves shall be used. The equipment required is a 1 ml glass pipette, a 100 ml glass-stoppered measuring flask and a device for spin casting. If a device for spin casting is not available, droplet deposition of the PC solution may be used. However, this will give poor repeatability, which will need to be carefully taken into account during spectral analysis Using poly(bisphenol A carbonate), abbreviated to PC, weigh out 100 mg on a clean piece of aluminium foil. Introduce the PC into the 100 ml, glass-stoppered measuring flask, add tetrahydrofuran (THF) of analytical reagent quality, to the 100 ml level line. Shake the flask to mix the PC and allow time to dissolve it completely. This produces a 1 mg/ml solution of PC in THF. The aluminium foil shall be freshly unrolled and the shiny surface used. Ensure that the THF is anhydrous. Otherwise, streaks will appear from water when spin coating as described in The shelf life of freshly prepared stock solution shall be no more than one month owing to water take-up. NOTE 1 It does not matter if the PC contains low levels of additives such as Irgafos. NOTE 2 It does not matter if the final PC/THF solution concentration varies by ±20 % Use a conveniently sized (1 cm by 1 cm) piece of silicon, or another flat or polished conducting substrate, and clean it overnight by soaking in propan-2-ol (isopropyl alcohol). Ultrasonically clean the substrate in fresh propan-2-ol and dry. If an ultrasonic bath is not available, just rinse the sample in fresh propan-2-ol. Mount the substrate on the spin casting device. Pipette approximately 0,2 ml of the PC solution onto the substrate and spin cast at r/min for 25 s. Samples may be prepared by depositing the PC solution using a 5 ml pipette onto the silicon surface then air drying under ambient conditions. However, this method will result in an uneven PC film, so care shall be taken when comparing spectra, as peak intensities will vary. NOTE 1 It is not essential what substrate is used, as long as it is conducting. Silicon has been found to give good-quality films. NOTE 2 Using this procedure, the film thickness will be approximately 10 nm. The absolute thickness is not critical. 4.3 Obtaining the SIMS spectral data Insert the PC sample inside the chamber of the SIMS instrument Operate the instrument in accordance with the manufacturer's or local documented instructions. The instrument shall have fully cooled following any bakeout. Ensure that the operation is within the manufacturer's recommended ranges for the ion-beam current, counting rates and any other parameter specified by the manufacturer. Check that the detector multiplier settings are correctly adjusted Select the normal analytical settings and acquisition time. For ToF instruments, select a repetition rate that gives a maximum mass of at least 800 u. If the total counts in the C 9 H 11 O peak are less than , increase the acquisition time to ensure that this peak contains more than counts. This may not be possible if the signal is too weak and it is not possible to achieve counts within a reasonable time. To ensure that the maximum ion fluence ( ions/m 2 ) is not exceeded, an enlarged raster area may be required. The acquisition time finally chosen will be a compromise between the data quality and the duration ISO 2011 All rights reserved 3

10 of the work. Record the parameters set. Ensure that the detector is not saturated using the manufacturer's or local documented instructions. This may be achieved by reducing the number of primary ions per pulse. NOTE For details of acquiring high-quality SIMS spectra with good repeatability and constancy, refer to ISO [1]. 4.4 Calculating mass accuracy Instrument manufacturers' software may provide the calculation of the peak position automatically; it is often sufficient to use this to obtain a value of M o. A more accurate and reliable method for measurement of the mass of the peak in the spectra, M o, can be used. An asymmetric Gaussian function, G A, can be used to fit to the signal intensity versus the mass position, M P, and the fitting used to calculate the peak position, M o. Where M o is the peak centre, M P is the peak mass and G o is a scaling term, G A, the fit to signal intensity, is given by 2 ( MP Mo) GA = Go exp 2[ ( 2 σ α MP Mo )] (1) and where FWHM( α = 0) σ = (2) 2 2ln2 FWHM(α = 0) is the full width at half-maximum of the base Gaussian width for α = 0. The term α gives the asymmetry, and for α = 0 the function is pure Gaussian. For each peak, fit Equation (1). Only use those intensities above 50 % of the maximum intensity to avoid interference from neighbouring peaks. You should calibrate using the peak position method you intend to use for accurate mass identification in your work. NOTE An asymmetric Gaussian function gives a good fit to a wide range of peak shapes, whereas the mean value can lead to significant errors for asymmetric peaks. Typically, the asymmetric Gaussian function is an excellent description of the peak down to 15 % of the maximum intensity, although the fitting, here, only covers to 50 % The mass accuracy, M, is defined as the difference between the measured peak mass, M P, and the true mass, M T M = MP M T (3) and the relative mass accuracy, W, is given by M W = (4) M T In the text that follows, W will be given in parts per million Figure 2 shows M for a range of hydrocarbon peaks of polycarbonate in an unoptimized instrument. M varies widely along the mass range for ions with different fragmentation. This illustrates an instrument with modest mass scale accuracy. 4 ISO 2011 All rights reserved

11 In Figure 2 the peaks marked with an arrow are used to calibrate the spectra. The circumscribed symbols denote the mass peaks used to measure σ M. Here the asymmetric Gaussian function is used. M, 10-3 u M, u Figure 2 Mass accuracy, M, for hydrocarbon peaks from PC positive-ion spectra with a reflector voltage, V R = 60 V To provide a statistical measure of the divergence of M from 0, select the peaks for the four well-defined C x H y + cascades with x = 4, 6, 7 and 8, respectively, identified in Figure 2 by the circumscribed data points and detailed in Table 1. Table 1 Peaks identified in Figure 1 used to calculate σ M x value Ion True mass, u 4 C 4 H 2 50, C 4 H 4 52, C 4 H 5 53, C 6 H 2 74, C 6 H 3 75, C 6 H 4 76, C 6 H 5 77, C 6 H 6 78, C 7 H 2 86, C 7 H 3 87, C 7 H 4 88, ISO 2011 All rights reserved 5

12 Table 1 (continued) x value Ion True mass, u 7 C 7 H 5 89, C 7 H 6 90, C 7 H 7 91, C 8 H 2 98, C 8 H 5 101, C 8 H 6 102, C 8 H 8 104, C 8 H 9 105, Measure M for each peak using Equation (3) and calculate the four standard deviations for σ Cx H y ( M), x = 4, 6, 7 and 8. The formula to calculate σ Cx H y ( M) is exampled for x = 6 in Equation (5). σ ( MC6H M y C6Hy ) C 6 H ( ) y= M = y 4 (5) Finally, calculate, σ M, the average of the standard deviations of M for each of the four C x H y + cascades defined in Table 1 using: 1 σ = σ ( M) + σ ( M) + σ ( M) + σ ( M) M C4H C6H C7H C8H 4 y y y y (6) where for x = 4, 6, 7 and 8, σ Cx H y ( M) is the standard deviation for the C x H y + cascade. NOTE Some care might be needed to take into account the lifetime of molecules and the changes this has on the mass accuracy. For the molecules used here, and shown in Table 1, there is no noticeable effect of the lifetimes of the molecules on the mass accuracy. 4.5 Optimizing instrumental parameters The measure σ M is now used to optimize the instrument operating parameters. For improved mass accuracy, the value of σ M needs to be minimized. This is illustrated with examples here, for a reflection instrument, for optimization of the lens settings and optimization of the analyser deflector X and Y plates, as shown in Figure 3. It is simple to locate the optimum lens setting from the minimum of the curve in Figure 3 a) giving a lens setting of 76 %. Similarly, it is clear that the optimum setting for the analyser deflector plates has a broad minimum, rising steeply at large deflections, centred approximately around a setting of 0 for both X and Y deflectors. It is therefore important that a suitable procedure is used to align the ion optical axis and the ion-beam raster area. This method may be used to optimize other parameters, such as energy slit values, contrast diaphragms, pass energy and extraction potential. Optimize these by conducting, iteratively, the procedures in 4.3 to 4.5 for a range of analyser settings, to obtain graphs similar to those in Figure 3. These can be used to decide which analyser settings will minimize σ M and hence give an optimum mass accuracy. Use guidance from the instrument operator's manual or the instrument manufacturers, to choose suitable variations in analyser settings. NOTE The optimization procedure aims to reduce the scatter seen in Figure 2. The scatter is characterized by the σ M value; a reduction of σ M is a reduction in that scatter. An example of the possible improvement in scatter is shown in Figure 3 as a reduction in σ M. The overall improvement will depend on the instrumental parameters that can be changed. 6 ISO 2011 All rights reserved

13 σ M, u ( 10-3 ) 2,5 2 1,5 1 0, X 1 a) Lens settings σ M, u ( 10-3 ) 2,5 2 y = 0 x = 0 1,5 1 0,5 0 X X 2 b) Analyser deflector X and Y settings Key X 1 lens setting, in % X 2 analyser deflector X and Y settings Figure 3 Change in σ M for different lens settings and analyser deflector X and Y settings ISO 2011 All rights reserved 7

14 4.6 Calibration procedure The mass calibration in ToF SIMS spectra is conducted in the spectrum itself, rather than the instrument being calibrated. In the measured spectrum, only peaks that you are confident in correctly identifying, shall be used as calibration peaks. NOTE Incorrectly identified peaks will lead to inaccuracies in the mass scale calibration; however, ensuring correct identification of peaks will negate this For samples exhibiting a roughness or edge height of over 1 µm, the mass resolution and mass scale calibration accuracy will be degraded. If the topography is structured (for example a MEMS device) rather than random (abraded surface), the mass calibration should be restricted to zones of similar sample height The true mass of the calibrant peaks shall be calculated using the identified molecular formula and a standard look-up table of atomic masses. Isotopic mass values, rather than average mass values, shall be used. In mass spectrometry, the ion is measured and therefore the mass of the electron (5, u) times the number of ionization charges should be subtracted or added for positive and negative ions respectively, for the relevant level of accuracy. NOTE For the example C 4 H 5 O: from a periodic table of isotope masses the commonest carbon (C) isotope is 12 and it has a mass of 12, u; similarly the mass of H = 1, u and the mass of O = 15, u. Therefore the true mass of the molecule C 4 H 5 O = 4 12 u + 5 1, u + 15, u = 69, u It is common practice to use hydrogen as the first mass in the calibration. This is very useful as it is easy to identify without a calibrated mass scale and may be used to establish a first calibration. However, for accurate calibration of the mass scale, hydrogen is not recommended. NOTE The uncertainty of the mass measurement of hydrogen is significantly greater than average. Part of the reason for this arises since the trajectory of hydrogen is affected more strongly by stray magnetic fields than heavier ions (often observed as a displacement of the ion image), thus adding to the uncertainty in the measured transit time and hence the deduced mass value For molecular analysis of minimally degraded fragments, use peaks for similarly minimally degraded entities as calibration peaks. That is: calibrate using ions that have low degradation or fragmentation from the original parent structure. Do not include atomic ions in the mass calibration. Avoid metastable ions. NOTE 1 Minimally degraded ions can be identified using G-SIMS (Reference [5] in the Bibliography). NOTE 2 Atomic ions have large kinetic energies, which lead to large values of M compared with organic ions. This biases the calibration. This arises since most mass spectrometers do not have full energy compensation. NOTE 3 Metastable ions can be identified by their broad peak shape Calibrate using a first mass m 1 within, or as close as possible to, the mass range 12 to 30 u and a second mass m 2 with as high a mass as is conveniently available. For identification of large molecules of mass m, include a mass m 2 0,55 m in the calibration ions. Some care may be needed to take into account the lifetime of molecules and the changes this has on the mass accuracy. The use of molecules with large peak widths that may indicate short lifetimes should be avoided. NOTE The requirement to use widely separated masses in the calibration, with m 2 0,55 m, is explained in Annex A Add several further intermediate calibration masses; five calibrant ions are sufficient. NOTE Using several measures generally improves the quality of the calibration. 8 ISO 2011 All rights reserved

15 Annex A (informative) Calibration uncertainty A.1 In the simplest case, the combined uncertainty, U(m), for a calibration using two peaks at masses m 1 and m 2, is given by [6]. 2 2 m2 m 2 m m1 2 Um ( ) = U1 + U2 m2 m1 m2 m1 1/ 2 (A.1) where the uncertainties U 1 and U 2 are the uncertainties in the accurate mass measurement of m 1 and m 2 respectively. For practical purposes, U 1 = U 2 = U 0 over most of the mass range of importance here. When m is equal to m 1 or m 2, this function gives U(m) = U 0 as expected from least-squares fitting and, when m is half way between m 1 and m 2, then U(m) = U 0 2. A.2 Figure A.1 shows the relative uncertainty U/U 0 using Equation (A.1) for five separate calibrations with m 1 = 10 and m 2 ranging from 100 to u. It is clear that the calibration uncertainty rises rapidly outside the calibration mass interval and, for a typical calibration interval with m 1 = 10 u and m 2 = 00 u, U/U 0 = 20 at m = u. For U 0 = u, this guarantees a relative mass accuracy, W, of 60 ppm. With m 1 = 10 u and m 2 = 500 u, it is found that U/U 0 = 2,3 at m = u, leading to an order of magnitude reduction in the relative mass accuracy, W, to 7 ppm. U/U m 2 = m, u Figure A.1 Relative uncertainties, U/U 0, using two calibration mass peaks illustrating the effect of extrapolation as a function of the given mass peak, m, up to u with m 1 = 10 and with separate curves for m 2 set at 100, 300, 500, and u ISO 2011 All rights reserved 9

16 Bibliography [1] ISO 23830, Surface chemical analysis Secondary-ion mass spectrometry Repeatability and constancy of the relative-intensity scale in static secondary-ion mass spectrometry [2] GILMORE, I S., SEAH, M P., GREEN, F M., Static TOF-SIMS A VAMAS Interlaboratory Study. Part I. Repeatability and Reproducibility of Spectra, Surface and Interface Analysis, 2005, 37, pp [3] GILMORE, I S., SEAH, M P., GREEN, F M., Static TOF-SIMS A VAMAS Interlaboratory Study. Part II. Accuracy of the mass scale and G-SIMS compatibility, Surface and Interface Analysis, 2007, 39, pp [4] GREEN, F M., GILMORE, I S., and SEAH, M P., ToF-SIMS: Accurate Mass Scale Calibration, Journal of the American Society of Mass Spectrometry, 2006, 17, pp [5] GILMORE, I S and SEAH, M P., Static SIMS: Towards unfragmented mass spectra The G-SIMS procedure, Applied Surface Science, 2000, 161, pp [6] SEAH, M P., GILMORE, I S., SPENCER, S J., XPS: Binding Energy Calibration of Electron Spectrometers 4 Assessment of Effects for Different X-ray Sources, Analyser Resolutions, Angles of Emission and of the Overall Uncertainties, Surface and Interface Analysis, 1998, 26, pp ISO 2011 All rights reserved

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